Rhodium‐Catalyzed Cyclization of Diynes with Nitrones: A Formal [2+2+5] Approach to Bridged Eight‐Membered Heterocycles

N‐aryl‐substituted nitrones were employed as five‐atom coupling partners in the rhodium‐catalyzed cyclization with diynes. In this reaction, the nitrone moiety served as a directing group for the catalytic C? H activation of the N‐aryl ring. This formal [2+2+5] approach allows rapid access to bridged eight‐membered heterocycles with broad substrate scope. The results of this study may provide new insight into the chemistry of nitrones and find applications in the synthesis of other heterocycles.     

加速溶剂萃取–液相色谱法测定五灵脂药材中原儿茶酸的含量

建立了五灵脂中原儿茶酸含量的测定方法。利用加速溶剂萃取仪(ASE),以75%乙醇水溶液提取样品中的待测物,用Diamosil C18(4.6 mm×250 mm,5.0μm)色谱柱在梯度洗脱条件下分离待测物,外标法定量。原儿茶酸的线性范围为0.1~10.0 mg/L,相关系数r=0.9998。方法的回收率为83%~107%,测定结果的相对标准偏差为4.6%~10.5%,方法的定量限为1.0 mg/kg。该方法操作简便、快速,提取效率高,适用于检测和分析五灵脂中原儿茶酸的含量。     

Enantioselective Alkynylzinc Addition to Carbonyl Compounds by Tf-based Sulfamide-amine Alcohol Catalysis

The new Tf‐based sulfamide‐amine alcohol 3a was found to be very effective in catalyzing the enantioselective alkynylzinc addition to both aromatic aldehydes and unactivated aromatic ketones without using another metal species under mild condition, providing up to 92% ee and 90% ee for aldehydes and ketones, respectively.     

波谱分析课程教学的实践与思考

介绍作者在长期波谱分析课程教学实践的基础上,对该课程教学内容及教学方法改革的一些探索。     

Optimal Conditions for Existence of Vesicles Under Electric Field

Giant vesicles have been of intense interest as the model system for cell membranes. To bring numerous applications of the vesicles into full play, the existence time of the vesicles becomes particularly important. In this work, we explored the existence time of the vesicles in distilled water under four kinds of representative alternative current (AC) electric fields with different energizing time. When the application time of AC electric field reached 1 hour, the existence time of the vesicles reached the maximum value. As the applied electric field time increased, the existence time of the vesicles decreased. Thus, after obtaining the best vesicles on the carbon fiber electrode, disconnecting the external electric field is very necessary. Based on the in situ observation using inverted microscope, the disappearing phenomena of the vesicles were presented. In addition, it is found that vesicles in phosphate buffer solutions (PBSs) can last about 2–3 days when the electric field was applied for 1 hour, which was much longer than that in distilled water.     

固体发动机保险机构在高温高压下的实验研究

针对固体发动机部件保险机构所出现破现象,对其进行了激光散斑和电阻应变法联合测试。由于保险机构在高温和高压环境下工作,材料有蠕变现象,出现较大的热变形,传统的光我法实施,发展了一种叠合散斑技术,使之能够对大变形进行非接触式测量,在实验室测试的基础上,对保险机构进行了热容器试验,测量了点火后应变随时间的变化规律。实验结构发现,在保险机构机体上存在着一个接近破环应力的高危应力区,这是保险机破坏的主要因素     

二羟基蒽醌磷酰化衍生物的合成及表征

分别以4种不同位取代的二羟基葸醌和亚磷酸二乙酯或亚磷酸二丙酯为原料,通过简化的Atheron-Todd合成法合成了一系列二羟基葸醌的磷酰化衍生物,并通过量化计算对葸醌上不同羟基电荷分布进行了研究,发现β-羟基氧上的电荷密度大于β-羟基氧上的电荷密度.所合成化合物的结构均经IR,MS,1H NMR,31p NMR和元素分析确证,并通过荧光猝灭法初步探讨了部分新化合物的生物活性.     

A new type of bis(sulfonamide)-diamine ligand for a Cu(OTf)2-catalyzed asymmetric Friedel-Crafts alkylation reaction of indoles with nitroalkenes

Chiral bis(sulfonamide)-diamine served as new type of ligand for a Cu(OTf)(2)-catalyzed asymmetric Friedel-Crafts alkylation reaction of indoles with nitroalkenes. The desired products were obtained with up to 99% yield and 97% ee.